CN106442512A - Detection kit for detecting diethylstilbestrol in food - Google Patents

Detection kit for detecting diethylstilbestrol in food Download PDF

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Publication number
CN106442512A
CN106442512A CN201611037547.4A CN201611037547A CN106442512A CN 106442512 A CN106442512 A CN 106442512A CN 201611037547 A CN201611037547 A CN 201611037547A CN 106442512 A CN106442512 A CN 106442512A
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China
Prior art keywords
test tube
food
diethylstilbestrol
detection kit
dehydrated alcohol
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CN201611037547.4A
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Chinese (zh)
Inventor
周朱晨
张根义
胡彬
张进
吴念绮
周合
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100 Olson Jiangsu Food Safety Technology Co Ltd
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100 Olson Jiangsu Food Safety Technology Co Ltd
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Priority to CN201611037547.4A priority Critical patent/CN106442512A/en
Publication of CN106442512A publication Critical patent/CN106442512A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a detection kit for detecting diethylstilbestrol in food. The detection kit comprises a kit body. At least one test tube provided with a plug and containing 5-8ml of anhydrous ethanol, at least one reagent bottle containing 2.5-3.0ml of concentrated sulfuric acid, at least one reagent bottle containing 2-3ml of anhydrous ethanol, at least one dry test tube provided with a plug and containing 10-12mg of vanillin, at least one 5ml disposable syringe and an organic-system microporous filter membrane are arranged in the kit body. The detection kit has the advantages that the detection kit is low in analyzing cost, high in specificity, high in sensitivity and suitable for fast detecting whether the food is mixed with the diethylstilbestrol or not on site, special equipment is not needed, and food supervision and inspection requirements are satisfied.

Description

The detection kit of diethylstilbestrol in a kind of food
Technical field
The present invention relates to technical field of food detection, the detection kit of diethylstilbestrol in specifically a kind of food.
Background technology
Diethylstilbestrol(Diethylstilbesrtol, DES)It is a kind of estrogen of synthetic, promoting uterus, defeated The aspect effect is significant such as oviduct, the growth promoter of mammary gland and protein synthesis, minimizing fat, raising daily gain, thus Zeng Zuowei During growth promoter produces for poultry, Aquatic product.However, many scientific investigations showed that DES can cause by changing hormonal system The cancer of humans and animals, can be with transplacental carcinogenesis, and that is, trimester of pregnancy use, may result in the distortion of fetus genitals, or even cancer Become.In addition, DES is difficult to degraded, such as excrete, understand severe contamination water source and soil, and human health is threatened by food chain And ecological environment, form vicious cycle.Therefore, China formulated in 1999《The People's Republic of China animal and animal-derived food Residue Monitoring plan》Middle regulation must not detect DES in animal derived food health, listed within 2002 again《Food animal The veterinary drug of disabling and its compound inventory》(The Ministry of Agriculture announces No. 193).However, ordering about due to huge interests, illegal interpolation The situation of DES still remains existing despite repeated prohibition, and seriously threatens human health.
At present, the DES detection method of document report mainly has chromatography(Gas chromatogram, gas chromatography-mass spectrography, height Effect liquid phase chromatogram etc.), immunization(Radioimmunology, enzyme linked immunosorbent assay, Chemiluminescence quantitative immunoassay)And fluorescence Spectrophotometer method, irradiation spectrophotography, bioanalysiss etc..High performance liquid chromatography and GC-MS Sensitivity is high, and result accurately and reliably, but is not suitable for the big field test of mobility, in vast rural area and underdeveloped Small and medium-sized cities carry out inspection activity have certain difficulty.
Content of the invention
It is an object of the invention to provide one kind is inexpensive, equipment is simple, specificity is strong, sensitivity is high, phenomenon is easy to see The detection kit of diethylstilbestrol in the food examined.
For achieving the above object, the present invention provides following technical scheme:
The detection kit of diethylstilbestrol in a kind of food, including box body;It is provided with least one in described box body and fill 5-8ml The tool plug test tube of dehydrated alcohol, at least one fills the reagent bottle of 2.5-3.0ml concentrated sulphuric acid, and it is anhydrous that at least one fills 2-3ml The reagent bottle of ethanol, at least one fills in test tube, the disposable injection of at least one 5ml equipped with the tool that is dried of 10-12mg vanillin Device, and organic system microporous filter membrane.
As the further scheme of the present invention:The concentration of described concentrated sulphuric acid is 4mol/L.
As the further scheme of the present invention:It is provided with the tool that at least one fills 6-7ml dehydrated alcohol in described box body Plug test tube, at least one fills the reagent bottle of 2.6-2.8ml concentrated sulphuric acid, and at least one fills the examination of 2.4-2.8ml dehydrated alcohol Agent bottle, at least one has plug test tube equipped with being dried of 11-11.5mg vanillin, the disposable syringe of at least one 5ml, and Organic system microporous filter membrane.
As the further scheme of the present invention:It is provided with the tool plug that at least one fills 6ml dehydrated alcohol in described box body Test tube, at least one fills the reagent bottle of 2.8ml concentrated sulphuric acid, and at least one fills the reagent bottle of 2.6ml dehydrated alcohol, and at least one Individual be dried tool plug test tube, the disposable syringe of at least one 5ml, and organic system micropore equipped with 11.2mg vanillin is filtered Film.
The method being detected using the detection kit of diethylstilbestrol in described food, is comprised the steps successively:
(1)Food samples 0.8-1.0g is taken to be placed in tool plug test tube, plus dehydrated alcohol, shake 2-3min, obtain sample crude extract;
(2)With organic system microporous filter membrane filtered sample crude extract, obtain test solution;
(3)Take test solution 2ml, add being dried in tool plug test tube equipped with 10-12mg vanillin, so that vanillin is dissolved;
(4)Add concentrated sulphuric acid in test tube, shaking is for several times;
(5)Test tube is placed in heating 2-3min in 78-82 DEG C of water-bath, so that dehydrated alcohol is volatilized, take out and let cool to room temperature;
(6)It is slowly added into dehydrated alcohol along test tube wall;
(7)Observe the color change of liquid level intersection and alcohol layer in 1min immediately.
As the further scheme of the present invention:Described step(7)In, observe liquid level intersection and ethanol in 1min immediately The color change of layer, should be add dehydrated alcohol after observe immediately, only need to gently rock test tube to the face that alcohol layer can be observed Color change, should not excessively shake makes two-layer too mix, and otherwise color is unfavorable for observing more deeply, determines showing of judged result As should be after adding dehydrated alcohol observed in 1min.
As the further scheme of the present invention:Described step(7)In, the criterion of color change is:If adding no In 1min after water-ethanol, the alcohol layer color of liquid layer intersection is first changed into purple, then is changed into violet or blueness, can tentatively conclude Containing diethylstilbestrol in sample, if not meeting this color change rule, or not observing this color change phenomenon in 1min, then For negative findings, parallel positive control test and blank assay should be carried out if necessary.
Compared with prior art, the invention has the beneficial effects as follows:
Analysis cost of the present invention is low, and specificity is strong it is not necessary to Special Equipment, sensitivity high it is adaptable to on-site rapid inspection food Whether mix diethylstilbestrol, meet the needs of food supervision and inspection, whether mix the special of diethylstilbestrol for inspection food simultaneously Laboratory provides quick screening method, to reduce analysis cost, to improve the purpose of checkability.Due to present invention test Phenomenon occurs in point liquid layer and upper strata alcohol layer, and colour developing is rapid and obvious, and therefore the present invention also has anti-coexisting substances interference Ability is strong, and substantially, check conclusion accuracy is high for phenomenon, easy and simple to handle quick it is not necessary to the advantages of using expensive instrument.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, Obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based in the present invention Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of not making creative work, all Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, the detection kit of diethylstilbestrol in a kind of food, including box body, in box body, it is provided with least one Fill the tool plug test tube of 5ml dehydrated alcohol, at least one fills the reagent bottle of the concentrated sulphuric acid that 2.5ml concentration is 4mol/L, at least One reagent bottle filling 2ml dehydrated alcohol, at least one fills in test tube, at least one 5ml equipped with the tool that is dried of 10mg vanillin Disposable syringe, and organic system microporous filter membrane.
The method being detected using the detection kit of diethylstilbestrol in described food, is comprised the steps successively:
(1)Food samples 0.8g is taken to be placed in tool plug test tube, plus dehydrated alcohol, shake 2min, obtain sample crude extract;
(2)With organic system microporous filter membrane filtered sample crude extract, obtain test solution;
(3)Take test solution 2ml, add being dried in tool plug test tube equipped with 10mg vanillin, so that vanillin is dissolved;
(4)Add concentrated sulphuric acid in test tube, shaking is for several times;
(5)Test tube is placed in heating 3min in 78 DEG C of water-bath, so that dehydrated alcohol is volatilized, take out and let cool to room temperature;
(6)It is slowly added into dehydrated alcohol along test tube wall;
(7)Observe the color change of liquid level intersection and alcohol layer in 1min immediately:If liquid layer in 1min after addition dehydrated alcohol The alcohol layer color of intersection is first changed into purple, then is changed into violet or blueness, tentatively can conclude in sample and contain diethylstilbestrol, If not meeting this color change rule, or in 1min, do not observe this color change phenomenon, then for negative findings, if necessary should Parallel carry out positive control test and blank assay.
Embodiment 2
In the embodiment of the present invention, the detection kit of diethylstilbestrol in a kind of food, including box body, in box body, it is provided with least one Fill the tool plug test tube of 8ml dehydrated alcohol, at least one fills the reagent bottle of the concentrated sulphuric acid that 3.0ml concentration is 4mol/L, at least One reagent bottle filling 3ml dehydrated alcohol, at least one fills in test tube, at least one 5ml equipped with the tool that is dried of 12mg vanillin Disposable syringe, and organic system microporous filter membrane.
The method being detected using the detection kit of diethylstilbestrol in described food, is comprised the steps successively:
(1)Food samples 1.0g is taken to be placed in tool plug test tube, plus dehydrated alcohol, shake 2-3min, obtain sample crude extract;
(2)With organic system microporous filter membrane filtered sample crude extract, obtain test solution;
(3)Take test solution 2ml, add being dried in tool plug test tube equipped with 12mg vanillin, so that vanillin is dissolved;
(4)Add concentrated sulphuric acid in test tube, shaking is for several times;
(5)Test tube is placed in heating 2min in 82 DEG C of water-bath, so that dehydrated alcohol is volatilized, take out and let cool to room temperature;
(6)It is slowly added into dehydrated alcohol along test tube wall;
(7)Observe the color change of liquid level intersection and alcohol layer in 1min immediately:If liquid layer in 1min after addition dehydrated alcohol The alcohol layer color of intersection is first changed into purple, then is changed into violet or blueness, tentatively can conclude in sample and contain diethylstilbestrol, If not meeting this color change rule, or in 1min, do not observe this color change phenomenon, then for negative findings, if necessary should Parallel carry out positive control test and blank assay.
Embodiment 3
In the embodiment of the present invention, the detection kit of diethylstilbestrol in a kind of food, including box body, in box body, it is provided with least one Fill the tool plug test tube of 6ml dehydrated alcohol, at least one fills the reagent bottle of 2.6ml concentrated sulphuric acid, and at least one fills 2.4ml no The reagent bottle of water-ethanol, at least one fills in test tube, the disposable injection of at least one 5ml equipped with the tool that is dried of 11mg vanillin Device, and organic system microporous filter membrane.
The method being detected using the detection kit of diethylstilbestrol in described food, same as Example 1.
Embodiment 4
In the embodiment of the present invention, the detection kit of diethylstilbestrol in a kind of food, including box body, in box body, it is provided with least one Fill the tool plug test tube of 7ml dehydrated alcohol, at least one fills the reagent bottle of 2.8ml concentrated sulphuric acid, and at least one fills 2.8ml no The reagent bottle of water-ethanol, at least one fills in test tube, the disposable injection of at least one 5ml equipped with the tool that is dried of 11.5mg vanillin Device, and organic system microporous filter membrane.
The method being detected using the detection kit of diethylstilbestrol in described food, same as Example 2.
Embodiment 5
In the embodiment of the present invention, the detection kit of diethylstilbestrol in a kind of food, including box body, in box body, it is provided with least one Fill the tool plug test tube of 6ml dehydrated alcohol, at least one fills the reagent bottle of 2.8ml concentrated sulphuric acid, and at least one fills 2.6ml no The reagent bottle of water-ethanol, at least one fills in test tube, the disposable injection of at least one 5ml equipped with the tool that is dried of 11.2mg vanillin Device, and organic system microporous filter membrane.
The method being detected using the detection kit of diethylstilbestrol in described food, is comprised the steps successively:
(1)Food samples 1.0g is taken to be placed in tool plug test tube, plus dehydrated alcohol, shake 3min, obtain sample crude extract;
(2)With organic system microporous filter membrane filtered sample crude extract, obtain test solution;
(3)Take test solution 2ml, add being dried in tool plug test tube equipped with 11.2mg vanillin, so that vanillin is dissolved;
(4)Add concentrated sulphuric acid in test tube, shaking is for several times;
(5)Test tube is placed in heating 3min in 80 DEG C of water-bath, so that dehydrated alcohol is volatilized, take out and let cool to room temperature;
(6)It is slowly added into dehydrated alcohol along test tube wall;
(7)Observe the color change of liquid level intersection and alcohol layer in 1min immediately:If liquid layer in 1min after addition dehydrated alcohol The alcohol layer color of intersection is first changed into purple, then is changed into violet or blueness, tentatively can conclude in sample and contain diethylstilbestrol, If not meeting this color change rule, or in 1min, do not observe this color change phenomenon, then for negative findings, if necessary should Parallel carry out positive control test and blank assay.
Analysis cost of the present invention is low, and specificity is strong it is not necessary to Special Equipment, sensitivity high it is adaptable to on-site rapid inspection Whether food mixes diethylstilbestrol, meets the needs of food supervision and inspection, whether mixes diethylstilbestrol for inspection food simultaneously Specialized laboratories provide quick screening method, to reduce analysis cost, to improve the purpose of checkability.Due to the present invention Experimental phenomena occurs in point liquid layer and upper strata alcohol layer, and colour developing is rapid and obvious, and therefore the present invention also has anti-coexisting substances Interference performance is strong, and substantially, check conclusion accuracy is high for phenomenon, easy and simple to handle quick it is not necessary to the advantages of using expensive instrument.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie In the case of the spirit or essential attributes of the present invention, the present invention can be realized in other specific forms.Therefore, no matter From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment only wraps Containing an independent technical scheme, only for clarity, those skilled in the art should for this narrating mode of description Using description as an entirety, the technical scheme in each embodiment can also form those skilled in the art through appropriately combined Understandable other embodiment.

Claims (4)

1. in a kind of food diethylstilbestrol detection kit, including box body;It is characterized in that, it is provided with least in described box body One tool plug test tube filling 5-8ml dehydrated alcohol, at least one fills the reagent bottle of 2.5-3.0ml concentrated sulphuric acid, at least one Fill the reagent bottle of 2-3ml dehydrated alcohol, at least one fills in test tube, at least one 5ml equipped with the tool that is dried of 10-12mg vanillin Disposable syringe, and organic system microporous filter membrane.
2. in food according to claim 1 the detection kit of diethylstilbestrol it is characterised in that described concentrated sulphuric acid Concentration is 4mol/L.
3. in food according to claim 1 the detection kit of diethylstilbestrol it is characterised in that setting in described box body At least one is had to fill the tool plug test tube of 6-7ml dehydrated alcohol, at least one fills the reagent bottle of 2.6-2.8ml concentrated sulphuric acid, extremely A few reagent bottle filling 2.4-2.8ml dehydrated alcohol, at least one tries equipped with the tool plug that is dried of 11-11.5mg vanillin Pipe, the disposable syringe of at least one 5ml, and organic system microporous filter membrane.
4. in food according to claim 3 the detection kit of diethylstilbestrol it is characterised in that setting in described box body At least one is had to fill the tool plug test tube of 6ml dehydrated alcohol, at least one fills the reagent bottle of 2.8ml concentrated sulphuric acid, at least one Fill the reagent bottle of 2.6ml dehydrated alcohol, at least one fills in test tube, at least one 5ml equipped with the tool that is dried of 11.2mg vanillin Disposable syringe, and organic system microporous filter membrane.
CN201611037547.4A 2016-11-23 2016-11-23 Detection kit for detecting diethylstilbestrol in food Pending CN106442512A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201535775U (en) * 2009-08-28 2010-07-28 北京望尔康泰生物技术有限公司 Stilboestrol ELISA detection regent kit
CN101799472A (en) * 2010-03-25 2010-08-11 中国农业科学院上海兽医研究所 Diethylstilbestrol detection kit and detection method
CN103616375A (en) * 2013-11-11 2014-03-05 江苏省食品药品检验所 Method and kit for detecting oxicams non-steroidal anti-inflammatory drugs in wind-damp expelling Chinese patent medicines and health-care foods

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201535775U (en) * 2009-08-28 2010-07-28 北京望尔康泰生物技术有限公司 Stilboestrol ELISA detection regent kit
CN101799472A (en) * 2010-03-25 2010-08-11 中国农业科学院上海兽医研究所 Diethylstilbestrol detection kit and detection method
CN103616375A (en) * 2013-11-11 2014-03-05 江苏省食品药品检验所 Method and kit for detecting oxicams non-steroidal anti-inflammatory drugs in wind-damp expelling Chinese patent medicines and health-care foods

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Application publication date: 20170222